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mbrown3391
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What does making NaNO2 from ammonia have to do with nitrogen trichloride?
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Dornier 335A
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I have tried synthesizing tiny amounts of NCl3 a number of times now. Every time the liquid has turned cloudy yellow (like in mbrown3391's
photos), but no drops have collected on the bottom. I have tried several processes including:
24% acetic acid mixed with 3% NaClO solution in 1:20, 1:10 and 1:1 volumetric ratios respectively, followed by addition of concentrated urea solution
drop by drop. Temperature was approximately 15°C.
NH4Cl dissolved in 24% acetic acid, followed by addition of 3% NaClO solution drop by drop. This was attempted at both 15°C and -5°C.
To make sure the acetic acid wasn't the problem, I switched to NaHSO4 solution as another weak acid and performed the above procedure
again, this time at -2°C.
Every time the yellow cloud forms when the solutions mix, but the solution turns clear, sometimes slightly yellow after some time, and almost
immediately if I swirl it around carefully.
I'm not sure how to continue from this. Am I doing some obvious mistake?
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TheChemiKid
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I tried making NCl3 once, I luckily did it in a fume hood with the hood down.
Long story short: My beaker blew up, and damaged the fume hood.
When the police come
\( * O * )/ ̿̿ ̿̿ ̿'̿'̵͇̿̿з=༼ ▀̿̿Ĺ̯̿̿▀̿ ̿ ༽
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Dornier 335A
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Then you obviously succeeded with making the NCl3 at least. What procedure did you use?
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The Volatile Chemist
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I attempted the [hydrochloric acid] acidified ammonium chloride solution and hypochlorite path, as well as adding ammonium chloride solution to
hydrochloric acid and adding manganese(IV) oxide to catalyze chlorine production, but neither have produced NCl3. For the first method, I
tried using many different concentrations of both acid, ammonia, and hypochlorite. Should I be using a lot more hypochlorite than the other two
reagents? Or should a little NCl3 form regardless?
For the second reaction, only copious amounts of chlorine were formed.
Are there any sure-fire methods that produce NCl3?
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franklyn
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electrolysis
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nitro-genes
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TCCA and ammonia salt, try extremely small amounts only
[Edited on 13-8-2015 by nitro-genes]
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blogfast25
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More scientific brilliance from the resident retard. And so well formatted too! 
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woelen
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To be more specific, electrolysis of a solution of NH4Cl with a platinum anode or graphite anode. At the
anode, NCl3 and HCl are formed. At the cathode you get H2 and NH3.
Avoid mixing of anode and cathode liquid. For small (demo) amounts, preventing mixing is not really necessary. You have to stop the process anyway if
you want to stay safe.
@franklyn: Why so terse?
[Edited on 13-8-15 by woelen]
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The Volatile Chemist
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I do have two graphite rods, is any high amperages needed? I'll have to work on a way to separate the solutions so it doesn't decay instantly.
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franklyn
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The quiddity (click) of what to search for — Googling NCl3 electrolysis , got me these. My cost 5 minutes.
http://nitrogen.atomistry.com/nitrogen_chloride.html
http://books.google.com/books?id=YtE5AQAAIAAJ&lpg=PA680&...
Revealing the mechanism of indirect ammonia electrooxidation
Attachment: Revealing the mechanism of indirect ammonia electrooxidation.pdf (644kB)
This file has been downloaded 1105 times
Obtained Googling NCl3 oil
http://www.lateralscience.co.uk/oil
http://projectseminars.org/report-risk-and-control-of-nitrog...
Instant gratification
http://www.youtube.com/watch?v=9A9Fg-hJy-4
Old bones , Duh
http://www.sciencemadness.org/talk/viewthread.php?tid=2079
Techniques to Disrupt, Deviate and Seize Control of
an Internet Forum In case you wonder W T F ! is going on here
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www.zerohedge.com/contributed/2012-10-28/cointelpro-techniques-dilution-misdirection-and-control-internet-forum https://web.archive.org/web/20120814124000/www.washingtonsblog.com/2012/08/the-15-rules-of-internet-disinformation.html
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S.C. Wack
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Good thing mbrown3391 didn't use a flash for his photo. His last login coming 2 weeks after his last posts starting a cyanide thread is duly noted;
well done.
Roscoe and Schorlemmer suggests clamping a large FBF full of Cl above a lead saucer in a bowl of a warm saturated solution of NH4Cl, in the hope that
NCl3 that collects on the flask all drops down and is collected.
Those who don't want to blow things up prepare solutions and use them right away. Inorg Syn used carbon tet with chloroform. Hentschel via JCS
Abstracts used benzene:
3000 c.c. of a solution of bleaching powder, containing 22.5 grams of active chlorine per 1000 c.c., is gently agitated in a stoppered flask of 5000
c.c. capacity, and cautiously treated with a 10 per cent. solution of hydrochloric acid until a portion of the solution no longer yields gas when
mixed with excess of a 20 per cent. solution of ammonium chloride. About 300 c.c. of the dilute acid is usually required for this purpose, and when
the proper quantity has been added, the liquid is treated with 300 c.c. of a 20 per cent. solution of ammonium chloride, and then vigorously agitated
with 300 c.c. of benzene during 30 seconds, the liquid meanwhile being protected from light; the benzene is separated from the aqueous liquid, and
transferred to a folded filter containing 20 grams of crushed calcium chloride.
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The Volatile Chemist
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OK, have some procedures to try, as soon as I finish up my chemistry summer work :/
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specialactivitieSK
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https://www.youtube.com/watch?v=kgvEn7l-ZZk
https://www.youtube.com/watch?v=9A9Fg-hJy-4
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The Volatile Chemist
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I'd seen both of these videos. The method in both of them doesn't appeal to me much, as I prefer small aqueous amounts free of as many ligands as
possible. I have a few experiments in mind that'd require such conditions.
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Velzee
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Quote: Originally posted by S.C. Wack  | Good thing mbrown3391 didn't use a flash for his photo. His last login coming 2 weeks after his last posts starting a cyanide thread is duly noted;
well done.
Roscoe and Schorlemmer suggests clamping a large FBF full of Cl above a lead saucer in a bowl of a warm saturated solution of NH4Cl, in the hope that
NCl3 that collects on the flask all drops down and is collected.
Those who don't want to blow things up prepare solutions and use them right away. Inorg Syn used carbon tet with chloroform. Hentschel via JCS
Abstracts used benzene:
3000 c.c. of a solution of bleaching powder, containing 22.5 grams of active chlorine per 1000 c.c., is gently agitated in a stoppered flask of 5000
c.c. capacity, and cautiously treated with a 10 per cent. solution of hydrochloric acid until a portion of the solution no longer yields gas when
mixed with excess of a 20 per cent. solution of ammonium chloride. About 300 c.c. of the dilute acid is usually required for this purpose, and when
the proper quantity has been added, the liquid is treated with 300 c.c. of a 20 per cent. solution of ammonium chloride, and then vigorously agitated
with 300 c.c. of benzene during 30 seconds, the liquid meanwhile being protected from light; the benzene is separated from the aqueous liquid, and
transferred to a folded filter containing 20 grams of crushed calcium chloride. |
You think he died(or was injured)?
Check out the ScienceMadness Wiki: http://www.sciencemadness.org/smwiki/index.php/Main_Page
"All truth passes through three stages. First, it is ridiculed. Second, it is violently opposed. Third, it is accepted as being self-evident."
—Arthur Schopenhauer
"¡Vivá Cristo Rey!"
—Saint José Sánchez del Río |
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S.C. Wack
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Odds are about even that, or he made it to appear so, or his chemical adventures aroused interest from the authorities, by one of the several ways
that could happen. His last posts were saying he was going to make HCN...maybe he used a flash for a NCl3 closeup instead. It looks like he's not
logging in any time soon, so we'll never know, that's the well done part.
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Sakomekieh
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I tried the synthesis using muriatic acid, sodium hypochlorite and ammonium salt(In this case Ammonium Bicarbonate), but no NCl3 formed... First i
reacted ammonium bicarbonate with excess muriatic acid, then mixed the solution with hypochlorite. The solution immediately turned green, but no NCl3
was formed.
I think that organic impurities in muriatic acid decomposed the NCl3(the smell of chlorine was really strong), but i'm not sure 
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The Volatile Chemist
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| Quote: Originally posted by Sakomekieh | I tried the synthesis using muriatic acid, sodium hypochlorite and ammonium salt(In this case Ammonium Bicarbonate), but no NCl3 formed... First i
reacted ammonium bicarbonate with excess muriatic acid, then mixed the solution with hypochlorite. The solution immediately turned green, but no NCl3
was formed.
I think that organic impurities in muriatic acid decomposed the NCl3(the smell of chlorine was really strong), but i'm not sure
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Eh, I tried it too. It's also possible the concentrations simply weren't strong enough. I had the exact same thing happen to me this summer.
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PHILOU Zrealone
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Better switch to more stable chloramines... see Axt tread about energetic haloamines... alkylic dichloroamines and dibromoamines...
CH3-NCl2
Cl2N-CH2-CH2-NCl2
Br2N-CH2-CH2-NBr2
PH Z (PHILOU Zrealone)
"Physic is all what never works; Chemistry is all what stinks and explodes!"-"Life that deadly disease, sexually transmitted."(W.Allen)
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The Volatile Chemist
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Why? Certainly if I wanted the NCl3 for an explosion, I would. But I want it for experimentation.
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PHILOU Zrealone
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What experimentation?
If you want to use it for safe experimentation it must be:
1°) In extremely low quantity (<1 drop)
2°) In diluted form
a) into a safe unreactive solvent (CCl4?)
b) into an inert dilutant gas
Manyfold of course!
PH Z (PHILOU Zrealone)
"Physic is all what never works; Chemistry is all what stinks and explodes!"-"Life that deadly disease, sexually transmitted."(W.Allen)
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The Volatile Chemist
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You know that's not what I'm planning, but I'm also not planning experimenting with more than a drop. Yes, it's explosive, but as long as I do the
experimentation outside, with physical protection, it doesn't seem like the other three things in your list are necessary. Just my opinion, for me,
though.
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PHILOU Zrealone
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Even a drop in glass, hard plastic or metal, may cause cutting or piercing schrapnels...
NCl3 has the bad habit to detonate upon contact with dirt, grease, almost anything can get a catalytic effect...
So take care of you with your physical protection.
PH Z (PHILOU Zrealone)
"Physic is all what never works; Chemistry is all what stinks and explodes!"-"Life that deadly disease, sexually transmitted."(W.Allen)
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The Volatile Chemist
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I will, though I doubt I'll get to look at it soon, as I have a lot of other things on my plate. I'll do it in the summer, outside, with protection
and such. If I do it at all.
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